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Triphenylphosphine → HCID 19779532、化合物

HRID 2082079
ノート
印刷プレビュー

反応式

HRID 2082079 の反応式
N(C(OCC)=O)=NC(OCC)=O.[CH3:13][C:14]1([CH2:19][O:20][C:21]2[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=2)[O:18][CH2:17][CH2:16][O:15]1.[C:28]([O:32][C:33]([NH:35][CH:36](O)[CH3:37])=[O:34])([CH3:31])([CH3:30])[CH3:29].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[C:28]([O:32][C:33]([NH:35][CH2:36][CH2:37][O:27][C:24]1[CH:25]=[CH:26][C:21]([O:20][CH2:19][C:14]2([CH3:13])[O:18][CH2:17][CH2:16][O:15]2)=[CH:22][CH:23]=1)=[O:34])([CH3:31])([CH3:30])[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 197795284-[(2-Methyl-1,3-dioxolan-2-yl)methoxy]phenolHCID 22620026t-Butoxycarbonylaminoethanol

生成物 1

HCID 19779532HCID 19779532、化合物収率 56%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

Diethyl azodicarboxylate (3.8 ml) was added dropwise to a stirred solution of 4-[(2-methyl-1,3-dioxolan-2-yl)methoxy]phenol (3.4 g), N-t-butoxycarbonylaminoethanol (5.2 g) and triphenylphosphine (6.3 g) in anhydrous tetrahydrofuran (100 ml), at ice-bath temperature, under argon. The reaction mixture was left for 64 hours at 25° C. and then the solvent was removed under reduced pressure. The residue was dissolved in ether (100 ml) and the ethereal solution washed with 2N aqueous sodium hydroxide (2×50 ml), water (2×50 ml) and saturated brine (50 ml). The aqueous washings were in turn extracted with ether (50 ml). The ethereal solutions were combined, dried, and the ether removed under reduced pressure. The residue was purified by chromatography using 11/2% tetrahydrofuran in dichloromethane as eluent. The appropriate fractions were combined and evaporated to yield 1-t-butoxycarbonylamino-2-[4-((2-methyl-1,3-dioxolan-2-yl)-methoxy)phenoxy]ethane as a light yellow solid (3.2 g) m.p. 80°-82° C. (from cyclohexane); microanalysis: found C, 61.3; H, 7.7; N, 3.8%; required for C18H27NO6 : C, 61.2; H, 7.6; N 4.0%.

後処理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in ether (100 ml)
  3. washthe ethereal solution washed with 2N aqueous sodium hydroxide (2×50 ml), water (2×50 ml) and saturated brine (50 ml)
  4. extractionextracted with ether (50 ml)
  5. customdried
  6. customthe ether removed under reduced pressure
  7. customThe residue was purified by chromatography
  8. customevaporated

出典と根拠

ORDレコード
ord-9988d3fbe2114963be2b3edc790cc57d
出典データセット
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05187190

反応ノート

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